CN106117610B - The preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film - Google Patents
The preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods for the full stalk regenerated cellulose active carbon nanoparticles plural gel film of corn for adsorbing heavy metal ion, the full stalk of air-dried corn is removed, is sheared by this method, grinding and screening, obtain two kinds of raw materials of stalk and leaf, stalk portion carries out oxygen/hydrogen peroxide/potassium hydroxide/anthraquinone processing, and cornstalk cellulose is made；Using low temperature lithium hydroxide（Sodium hydroxide）/ thiocarbamide（Urea）Method dissolves cellulose；Using heating carbonization, ball milling, Ethanol activation dispersion and centrifugal classification, maize leaves are converted into active carbon nanoparticles；Above-mentioned activated carbon with stalk portion cellulose dissolution liquid is mixed, in die forming, sulfuric acid bath and shapes, wash, is dry, obtaining the full stalk plural gel film of corn.It is translucent brown sheet by gel mould made from this method, to Zn2+、Fe3+、Cd3+And Cu2+Etc. heavy metal ion have higher adsorption capacity.
Description
Technical field
Agricultural solid residue is utilized the present invention relates to a kind of --- the full stalk of corn prepares the natural of high absorption heavy metal ion
The technology of Macromolecule glued membrane belongs to natural macromolecule modification field of material technology.
Background technology
Heavy Metal Pollution in Water Environment, it has been more than the self-purification capacity of water body to refer to the heavy metal classes pollutant for being discharged into water body, is made
The composition and its property of water are changed, so as to deteriorate growth conditions biological in water environment, to human lives and health
Generate dysgenic behavior[1].In recent years, it is domestic or external, with industrial or agricultural and the fast development of economy, water
Heavy Metals In Environment is on the rise.The discharge of waste water containing heavy metal ion is to cause environmental pollution, and particularly water is dirty
One main source of dye, have carcinogenic, teratogenesis, the harm such as disable heavy metal wastewater thereby, the mankind are produced with very big danger
Evil.The main source of Heavy Metals in Waters pollutant is mining, metal smelt, intermetallic composite coating and chemical production wastewater, change
Burning, applying pesticides chemical fertilizer and house refuse of stone fuel etc., the wherein pollutant of Heavy Metals include copper, zinc, cadmium, chromium,
Iron, lead etc..
Two approach are broadly divided into the removal of the heavy metal ion in water：1）It reduces heavy metal and migrates energy in water body
Power and bioavailability；2）Heavy metal is thoroughly removed from water body[2].Currently used processing method has Physical（It inhales
Attached method, hyperfiltration and electroosmose process etc.）, chemical method（The precipitation method, oxidation-reduction method, electrolysis etc.）And bioanalysis（Plant method,
Animal law and microbial method etc.）, wherein physisorphtion is the method for more typical low dense removal of heavy metal ions[3].Activated carbon
It is as raw material, such as sawdust, waste paper, bamboo, coconut husk etc., through hydrophobicity made from high temperature cabonization and activation by carbon containing substance
Adsorbent.It is a kind of relatively effective heavy metal ion adsorbing material that numerous experimental studies, which is proved activated carbon,[4-6].It is same with this
When, cellulose is now extensive with recyclability because its resource amount of storage is big as one of main high molecular component of plant
Ground develops and utilizes.According to domestic and international relevant report, there are a large amount of microcellular structures for regenerated cellulose gel（Pore diameter range 50~
Within 100nm）, and with larger specific surface area（300~400m2/g）, it is adsorbable and carry a large amount of heavy metal ion, be
Excellent sorbing material[7].But because of the gel mould physical strength that natural or regenerated cellulose is formed, such as draftability and is torn damage resistibility
Fragility is poor, is greatly limited in practical applications.In order to overcome such defect, prepare cellulose gel film and usually require
Chemical crosslinking, but product cost and the complexity of operating procedure are increased, on the other hand, now for cellulose crosslinked examination
Agent[8]Basic source proposes query in petrochemicals, natural sex and degradability for gel products.Therefore, this hair
Bright patent is put forward for the first time by being blended with nano level active charcoal, to promote the physical strength of regenerated cellulose film, meanwhile, this side
Method can also strengthen the adsorption effect of product heavy metal ion.
In the scope of natural macromolecule modification research, activated carbon and cellulose are mainly derived from plant material, nature
The type of middle plant is various, and the stock number of various plants is not quite similar, the component and structure in different plant materials also differ compared with
Greatly, then, the raw material that selection is suitable for gel film preparation in numerous floristics is the underlying issue of the application.
Cornstalk is one of three big stalk resource of China, and annual output can reach 2.5 hundred million~3.0 hundred million tons[9].With resource height
The continuous propulsion utilized is imitated, the research of cornstalk is gradually increased, higher value application has obtained more concerns.The full stalk of corn
Including stalk portion（Bast and marrow core）And leaf, wherein, abundant carbohydrate is contained in stalk（Cellulose and half fiber
It is respectively 31.09% and 31.22% to tie up cellulose content）[10], prove that maize straw can be used as cellulose function material from raw material components
The initial feed of material.In addition, maize leaves are mainly made of epidermal tissue, spongy tissue and palisade tissue[11], because of its tissue
Cell has the functional characteristic of storage nutriment, determines that total sugar content is higher in maize leaves（66.15%）[12], in corn
The phosphorus content highest of leaf portion in full stalk；In addition, number of crystals fine and close in maize leaves soft texture, porosity height and cellulose
Measure it is relatively fewer, thus, maize leaves in terms of active carbon nanoparticles are prepared have stronger advantage.
The heavy metal pollution of water body problem with reference to caused by modern industry, the application is described in detail prepares height by raw material of the full stalk of corn
The technological process of effect absorption heavy metal ion regenerated cellulose composite Nano activated carbon gel mould.Corn resources can not only be improved
Comprehensive utilization ratio, and the high value added utilization for the full stalk of corn provides foundation.
Bibliography
[1] J.J.Chen, A.L.Ahmad, B.S.Ooi.Thermo-responsive properties of poly
(N-isopropylacrylamide-co-acrylic acid) hydrogel and its effect on copper ion
removal and fouling of polymer-enhanced ultrafiltration [J]. Journal of
Membrane Science, 2014, 469: 73-79.
[2] development [D] the Jinan of the clean heavy metal wastewater therebies purification seperation films of Lu Xing：University Of Ji'nan, 2014.
[3] preparation of the molecular sieve filled poly (ether sulfone) film adsorbents of the new .4A of Sun Jian and Study on adsorption properties [D] Tianjin：My god
Tianjin polytechnical university, 2013.
[4] Z.Z.Guo, J.L.Fan, J.Zhang, Y.Kang, H.Liu, L.Jiang, C.L.Zhang.
Sorption heavy metal ions by activated carbons with well-developed
microporosity and amino groups derived from Phragmites australis by ammonium
phosphates activation [J]. Journal of the Taiwan Instituted of Chemical
Engineers, 2016, 58: 290-296.
[5] X.S. Luo, Z.Zhang, P.X.Zhou, Y.N.Liu, G.F.Ma, Z.Q.Lei. Synergic
adsorption of acid blue 80 and heavy metal ions (Cu2+/Ni2+) onto activated
carbon and its mechanisms [J]. Journal of Industrial and Engineering
Chemistry, 2015, 27:164-174.
[6] H. Tounsadi, A. Khalidi, M. Abdennouri, N. Barka. Activated
carbon from Diplotaxis Harra biomass: Optimization of preparation conditions
and heavy metal removal [J]. Journal of the Taiwan Instituted of Chemical
Engineers, 2016, 59: 348-358.
[7] N. Isobe, X.X. Chen, U.J. Kim, et al. TEMPO-oxidized cellulose
hydrogel as high-capacity and reusable heavy metal ion adsorbent [J]. Journal
of Hazardous Materials, 2013, 260: 195-201.
[8] Tian Lingyuan, Wu Ronglan, Xu Shimei wait celluloses-g-p (4Vp/MBA) copolymer homogeneously to prepare and apply
Research ［ J ］ functional materials, 2013,（z2）：311-315.
[9] yellow thinking, Zhou Dingguo, the extraction of Wu Qing woods maize leaves nano-celluloses and characterization [J] China papermaking
Report, 2015,30（3）：1-4.
[10] Liu Liying, Chen Hong chapter maize straw component near-infrared diffusing reflections（NIRS）Foundation ［ J ］ light of assay method
Spectroscopy and spectrum analysis, 2007,27（2）：275-278.
[11] plant leaf image retrievals of the Shenyang city based on character and cluster research [D] Xiamen：Xiamen University,
2006.
[12] Yin Shan corals corn biomass adsorbent is to absorption research [D] the Shanghai of Pb in aqueous solution (II)：Eastern Hua Da
It learns, 2015.
Invention content
Since heavy metal adsorption film depends on synthesis class or semi-synthetic family macromolecule, using natural polymer as whole bases
The exploitation of the adsorbent of matter has both environmentally friendly and good physical behavior there are no enough bases and the support of technology
Adsorbed film do not have not been reported also and development and application.Therefore, the present invention provides a kind of high absorption heavy metal ion regenerated fibers
The preparation method of element-activated carbon plural gel film, this method are original using the still shallow full stalk of corn of resourceful but Exploitation Depth
Material, heating carbonization maize leaves, grinding, ethyl alcohol, which impregnate, to be disperseed and forms active carbon nanoparticles after drying, meanwhile, the fibre in extraction stalk portion
Activated carbon is dispersed in lysate, prepares the composite regenerated cellulose gel film of activated carbon, further open up by dimension element, dissolving
The application field of the full stalk of corn is opened up, this green recyclable materials of stalk is made to obtain the utilization of high added value.
Realize that the process technology scheme that the object of the invention is taken is as follows：
1. the full stalk of corn carries out leaf and stalk separation after air-drying, leaf, stalk two parts are not sheared, grind and sieving at
Reason, obtains acceptable material；
2. stalk portion raw material carries out oxygen/hydrogen peroxide/potassium hydroxide/anthraquinone processing under given conditions, after being disposed,
Slurry is impregnated, disperses and washed with deionized water repeatedly, until washings are neutrality, is obtained after filtering out excessive moisture using filter
It is spare to cornstalk cellulose；
3. using lithium hydroxide（Sodium hydroxide）/ thiocarbamide（Urea）Technology, under cryogenic to cornstalk cellulose into
Row mechanical agitation dissolution process, lysate removes air and undissolved cellulose in liquid by centrifugation, after being cleaned
Cellulose dissolution liquid, it is spare；
4. the maize leaves heating carbonization after sieving, the carbonization leaf after ball milling continue heating and are carbonized, ethyl alcohol immersion dispersion,
It centrifuges, collects supernatant, be dried to obtain active carbon nanoparticles；
5. active carbon nanoparticles and the stalk portion cellulose dissolution liquid of step 3. are mixed in a certain ratio uniformly, it is a certain amount of mixed
It closes liquid to pour into mold, and a period of time is submerged in certain density sulfuric acid bath, formed and coagulate solid gel mould, sample is used
Deionized water is washed repeatedly, and freeze-drying obtains the full stalk regenerated cellulose active carbon nanoparticles plural gel film of sheet corn.
The preparation method of regenerated cellulose-active carbon nanoparticles plural gel film of present invention absorption heavy metal ion, specifically
Operation is as follows：
1. the melting process of the full stalk of corn:The full stalk of corn is after air-drying processing, wherein air-drying the moisture of raw material according to not
Different and different with season air humidity from different places, for general moisture control in the range of 5~25%, air dry matter carries out leaf
With stalk lift-off processing, and crush after with 40~400 the polished standard screens screening, be able to powdered leaf and stalk two parts raw material；
2. cellulose extraction process:Cornstalk after screening and potassium hydroxide, hydrogen peroxide, anthraquinone are sufficiently mixed stirring
After uniformly, it is transferred to oxygen completely and takes off tank（Sealed pressure vessel tank）In, addition deionized water adjusts dense to desired material processing
Degree, after carrying out 60~300s of oxygenation under certain pressure requirement, sealing is put into rotatable heater and is reacted；React item
Part is:Potassium hydroxide dosage is the 20.0~50.0% of over dry material quality, and hydrogen peroxide use is over dry material quality
10.0~35.0%, anthraquinone dosage be over dry material quality 0.05~0.5%, 0.1~0.8MPa of oxygen pressure, material processing
Mass percent concentration 8.0~15.0%, 5.0~15.0h of reaction time, 100~160 DEG C for the treatment of temperature；After being disposed
Slurry takes off from oxygen to be transferred in tank completely in 300~600 mesh slurry bag, is impregnated, washed using deionized water, until washings
PH value centrifuges removing excessive moisture, makes slurry mass dryness fraction in the range of 10.0~30.0% in the range of 6.0~8.0, standby
With；
Magnesium sulfate alternative is added in above-mentioned steps, and magnesium sulfate dosage is the 0.0~1.0% of over dry material quality, and
Not equal to 0%.
3. cornstalk cellulose dissolution process:First by lithium hydroxide（Sodium hydroxide）And thiocarbamide（Urea）It is dissolved in the water,
Make lithium hydroxide in aqueous solution（Sodium hydroxide）A concentration of 2.5~6.0%（Mass percent）, thiocarbamide（Urea）A concentration of 8~
25%（Mass percent）, after aqueous solution is cooled to -20~-10 DEG C, cornstalk cellulose and 8~30min of high degree of agitation are added in,
Wherein, the volume ratio of cornstalk cellulose absolute dry mass and solution after cooling is 1g:10mL~1g:100mL, cellulose dissolution liquid
10~30min is centrifuged under 7000~15000rpm, removes undissolved cellulose and bubble, collects cellulose dissolution liquid；
4. the process for preparing maize leaves active carbon nanoparticles is as follows:The maize leaves of crushing heat in 150~300 DEG C of Muffle furnaces
0.5~3.0h, material be cooled to room temperature after using 12~72h of ball milling, continue in 150~300 DEG C of Muffle furnaces heating 2~
12h after material is cooled to room temperature again in drier, is scattered in absolute ethyl alcohol, 24~72h of magnetic agitation, wherein material
Quality is 10mg with absolute ethyl alcohol volume ratio:1mL~1mg:1mL；After the completion of immersion under 7000~15000rpm centrifugation 15~
35min collects supernatant, dry, obtains active carbon nanoparticles；
5. the realization process of the full stalk regenerated cellulose-carbon nano-fiber gel mould of corn:By active carbon nanoparticles and step 3.
Cornstalk cellulose lysate 1mg in proportion:10mL~1mg:200mL is uniformly mixed, mixed liquor is poured into a diameter of 5~
20mm, depth are in the mold of 0.1~1mm, and the mold equipped with mixed liquor soaks in the sulfuric acid bath of mass percent concentration 5~20%
Solidifying solid gel mould is removed from the molds, is washed repeatedly with deionized water by not 10~180min, and freeze-drying obtains
To the full stalk regenerated cellulose active carbon nanoparticles blended gel film of round corn.
The beneficial effects of the invention are as follows：With the stalk portion in the full stalk of agricultural wastes corn（Bast and marrow core）With leaf portion conduct
The source of cellulose and activated carbon, passes through lithium hydroxide（Sodium hydroxide）/ thiocarbamide（Urea）Technology dissolution in low temperature stalk portion cellulose,
Maize leaves high temperature cabonization simultaneously, ball milling, again high temperature cabonization, then ethyl alcohol dispersion centrifuge, gained active carbon nanoparticles
It is mixed with above-mentioned stalk portion cellulose dissolution liquid, the heavy full stalk regenerated cellulose blending nanometer of corn for obtaining absorption heavy metal ion of acid
Activated carbon gel mould.Natural polymer subclass attractive gel have synthesis high score subclass sorbing material general character, can mining,
It can be played in terms of the processing of heavy metal waste liquid caused by multiple industries such as metallurgy, machine-building, chemical industry, electronics and instrument good
Good application prospect.Meanwhile the natural polymer subbase attractive gel film is also equipped with hypotoxicity, good absorption property, environment friend
The advantages such as good property and cheap price are novel, the green functional materials of one kind of mainstream development now, such adsorbed film
It is embodied as the full stalk high value added utilization of corn and one feasible scheme is provided, the functionalization exploitation that stalk is also abandoned for other agricultures provides
Certain basis early period.
Specific embodiment
The present invention is described in further detail with reference to embodiment, but the scope of the present invention is not limited in described
Hold.
Embodiment 1：The preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film, concrete operations are such as
Under：
（1）The melting process of maize straw
Stalk is by air-drying processing, wherein the water content for air-drying raw material is 5%, then air dry matter is carried out at leaf and stalk stripping
Reason, two parts raw material are crushed, are sieved with standard screen respectively, take 40 mesh screens, but only the part of 60 mesh screens is two kinds of conjunctions
Lattice raw material.
（2）The extraction process of cellulose
Cellulose separation condition is:Potassium hydroxide dosage 20.0%, hydrogen peroxide use 10.0%, does not add magnesium sulfate,
Anthraquinone dosage 0.05%, oxygen pressure 0.1MPa, material concentration for the treatment of 8.0%, reaction time 5.0h, 160 DEG C for the treatment of temperature.
The specific steps are:By the over dry cornstalk powder raw material of 10.0g（If it is 5.00% to air-dry raw material moisture, claim
10.5g is taken to air-dry material）With 10.0mL potassium hydroxide solutions（Concentration 200.0g/L), 12.5mL hydrogenperoxide steam generators（Concentration 80g/
L）, 0mL Adlerikas（Concentration 50g/L) and 0.005g anthraquinones mixing stir, adding in total deionized water volume is
Mixed material is transferred to oxygen and takes off tank by 92.0mL completely（Sealed pressure vessel tank）In, 0.1MPa oxygen pressures amount oxygenation 60s
Afterwards, it seals, is put into rotatable heater, the primary delignification reaction 5.0h under the conditions of 160 DEG C；
Slurry after being disposed（That is gained cornstalk cellulose）It takes off and is transferred to completely in tank in 300 mesh slurry bag from oxygen,
Deionized water immersion, washing are carried out, until washings pH value is 6.0, it is pulp centrifuged after cleaning to slough excessive moisture, make cellulose
Mass dryness fraction is about 10.0% or so.
（3）Cornstalk cellulose course of dissolution
Cellulose dissolution condition is:Lithium hydroxide a concentration of 2.5% in lysate, thiourea concentration 8%, lysate is first cold
But to -10 DEG C, the volume ratio of bone dry fiber quality amount and lysate is 1g:10mL.
Specifically dissolving step is:1.25g lithium hydroxides and 4g thiocarbamides are weighed, and 5mL water mixed dissolutions, after dissolving
It is put into refrigerating chamber and lysate is cooled to -10 DEG C, be put into 5g over dry cornstalk celluloses（Cellulose mass dryness fraction is 10%, therefore is taken
5/10%=50g cornstalk celluloses, wherein 45g are the weight of water）High degree of agitation 30min, makes cellulose fully be dissolved,
Dissolved cellulose solution centrifuges 10min under 7000rpm, collects supernatant, obtains cornstalk cellulose lysate.
（4）The preparation of maize leaves active carbon nanoparticles
Maize leaves powder is carbonized 0.5h in 150 DEG C of Muffle furnaces, carbide be cooled to room temperature after using ball milling 12h,
Continuing the 2h that is carbonized in 150 DEG C of Muffle furnaces, carbonization material in drier is cooled to room temperature, is scattered in absolute ethyl alcohol again,
For 24 hours, wherein quality of material and absolute ethyl alcohol volume ratio are 10mg to magnetic agitation:1mL；It is centrifuged under 7000rpm after the completion of immersion
15min collects supernatant, dry, obtains active carbon nanoparticles.
（5）The preparation of the full stalk regenerated cellulose of corn-active carbon nanoparticles blended gel film
Take step（4）In 1mg active carbon nanoparticles and 10mL steps（3）In cellulose dissolution liquid be uniformly mixed（The two
Than for 1mg:10mL）, a diameter of 5mm is poured into, depth is in the mold of 0.1mm, by the mold equipped with mixed liquor in 5% sulfuric acid bath
10min is submerged, sample gradually forms solidifying solid gel mould by viscous liquid, and film is removed from the molds, and is carried out with deionized water
It washs, is freeze-dried repeatedly, obtain the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of round corn.
（6）The character of the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of corn
Adsorption of metal ions assay method:It is a concentration of that the desiccant gel film of measure access 50mg is immersed in 1mL respectively
The Zn of 1mg/mL2+、Fe3+、Cd3+And Cu2+In standard solution, 72h is stood under 25 DEG C of water temperatures, after adsorption equilibrium, take out film, wipe
It wipes film surface layer liquid away, the content of beary metal adsorbed in film is detected using elemental analyser.
Blended gel film as obtained by above-mentioned reaction has higher metal adsorption capacity, to Zn2+、Fe3+、Cd3+And Cu2+
Adsorption capacity respectively reaches 330mg/g, 116mg/g, 252mg/g and 370mg/g.
Embodiment 2：It is specific to grasp based on the preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film
Make as follows：
（1）The melting process of maize straw
Stalk is by air-drying processing, wherein the water content for air-drying raw material is 15%, then air dry matter carries out leaf and stalk stripping
Processing, two parts raw material are crushed, are sieved with standard screen, take and sieve with 100 mesh sieve net respectively, but only the part of 200 mesh screens is two
Kind acceptable material.
（2）The extraction process of cellulose
Cellulose separation condition is:Potassium hydroxide dosage 30.0%, hydrogen peroxide use 20.0%, magnesium sulfate dosage
0.5%, anthraquinone dosage 0.25%, oxygen pressure 0.6MPa, material concentration for the treatment of 12.0%, reaction time 10.0h, treatment temperature
130℃。
The specific steps are:By the over dry cornstalk powder raw material of 10.0g（If it is 15.00% to air-dry raw material moisture, claim
11.8g is taken to air-dry material）With 15.0mL potassium hydroxide solutions（Concentration 200.0g/L), 25.0mL hydrogenperoxide steam generators（Concentration 80g/
L）, 1.0mL Adlerikas（Concentration 50g/L) and 0.025g anthraquinones mixing stir, add in total deionized water volume
For 30.5mL, mixed material is transferred to oxygen completely and takes off tank（Sealed pressure vessel tank）In, the oxygenation of 0.6MPa oxygen pressures amount
After 200s, sealing is put into rotatable heater, the primary delignification reaction 10.0h under the conditions of 130 DEG C；
Slurry after being disposed（That is gained cornstalk cellulose）It takes off and is transferred to completely in tank in 500 mesh slurry bag from oxygen,
Deionized water immersion, washing are carried out, until washings pH value is 7.0, it is pulp centrifuged after cleaning to slough excessive moisture, make cellulose
Mass dryness fraction is about 20.0% or so.
（3）Cornstalk cellulose course of dissolution
Cellulose dissolution condition is:Lithium hydroxide a concentration of 4.0% in lysate, thiourea concentration 15%, lysate are first
It is cooled to -15 DEG C, the volume ratio of bone dry fiber quality amount and lysate is 1g:50mL.
Specifically dissolving step is:10.0g lithium hydroxides and 37.5g thiocarbamides are weighed, with 230mL water mixed dissolutions, dissolving
After be put into refrigerating chamber lysate be cooled to -15 DEG C, be put into 5g over dry cornstalk celluloses（Cellulose mass dryness fraction is
20%, therefore 5/20%=25g cornstalk celluloses are taken, wherein 20g is the weight of water）High degree of agitation 20min, make cellulose into
Row fully dissolving, dissolved cellulose solution centrifuge 10min under 7000rpm, collect supernatant, it is molten to obtain cornstalk cellulose
Solve liquid.
（4）The preparation of maize leaves active carbon nanoparticles
Maize leaves powder is carbonized 2.0h in 250 DEG C of Muffle furnaces, carbide be cooled to room temperature after using ball milling 48h,
Continuing the 8h that is carbonized in 250 DEG C of Muffle furnaces, carbonization material in drier is cooled to room temperature, is scattered in absolute ethyl alcohol again,
Magnetic agitation 48h, wherein quality of material are 5mg with absolute ethyl alcohol volume ratio:1mL；It is centrifuged under 10000rpm after the completion of immersion
25min collects supernatant, dry, obtains active carbon nanoparticles.
（5）The preparation of the full stalk regenerated cellulose of corn-active carbon nanoparticles blended gel film
Take step（4）In 1mg active carbon nanoparticles and 100mL steps（3）In cellulose dissolution liquid be uniformly mixed（The two
Than for 1mg:100mL）, a diameter of 15mm is poured into, depth is in the mold of 0.6mm, by the mold equipped with mixed liquor in 10% sulfuric acid
100min is submerged in bath, sample gradually forms solidifying solid gel mould by viscous liquid, and film is removed from the molds, and uses deionized water
It is washed, is freeze-dried repeatedly, obtain the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of round corn.
（6）The character of the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of corn
Adsorption of metal ions assay method:It is a concentration of that the desiccant gel film of measure access 50mg is immersed in 1mL respectively
The Zn of 1mg/mL2+、Fe3+、Cd3+And Cu2+In standard solution, 72h is stood under 25 DEG C of water temperatures, after adsorption equilibrium, take out film, wipe
It wipes film surface layer liquid away, the content of beary metal adsorbed in film is detected using elemental analyser.
Blended gel film as obtained by above-mentioned reaction has higher metal adsorption capacity, to Zn2+、Fe3+、Cd3+And Cu2+
Adsorption capacity respectively reaches 511mg/g, 372mg/g, 318mg/g and 495mg/g.
Embodiment 3：It is specific to grasp based on the preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film
Make as follows：
（1）The melting process of maize straw
Stalk is by air-drying processing, wherein the water content for air-drying raw material is 25%, then air dry matter carries out leaf and stalk stripping
Processing, two parts raw material are crushed, are sieved with standard screen respectively, take 200 mesh screens, but only the part of 400 mesh screens is two
Kind acceptable material.
（2）The extraction process of cellulose
Cellulose separation condition is:Potassium hydroxide dosage 50.0%, hydrogen peroxide use 35.0%, magnesium sulfate dosage
1.0%, anthraquinone dosage 0.5%, oxygen pressure 0.8MPa, material concentration for the treatment of 15.0%, reaction time 15.0h, treatment temperature
100℃。
The specific steps are:By the over dry cornstalk powder raw material of 10.0g（If it is 25.00% to air-dry raw material moisture, claim
13.3g is taken to air-dry material）With 20.0mL potassium hydroxide solutions（Concentration 250.0g/L), 29.2mL hydrogenperoxide steam generators（Concentration 120g/
L）, 2.0mL Adlerikas（Concentration 50g/L) and 0.05g anthraquinones mixing stir, adding in total deionized water volume is
Mixed material is transferred to oxygen and takes off tank by 2.2mL completely（Sealed pressure vessel tank）In, 0.8MPa oxygen pressures amount oxygenation 300s
Afterwards, it seals, is put into rotatable heater, the primary delignification reaction 15.0h under the conditions of 100 DEG C；
Slurry after being disposed（That is gained cornstalk cellulose）It takes off and is transferred to completely in tank in 600 mesh slurry bag from oxygen,
Deionized water immersion, washing are carried out, until washings pH value is 8.0, it is pulp centrifuged after cleaning to slough excessive moisture, make cellulose
Mass dryness fraction is about 30.0% or so.
（3）Cornstalk cellulose course of dissolution
Cellulose dissolution condition is:Lithium hydroxide a concentration of 6.0% in lysate, thiourea concentration 25%, lysate are first
It is cooled to -20 DEG C, the volume ratio of bone dry fiber quality amount and lysate is 1g:100mL.
Specifically dissolving step is:30.0g lithium hydroxides and 125.0g thiocarbamides are weighed, mixes, has dissolved with 488.3mL water
Refrigerating chamber is put into after finishing, lysate is cooled to -20 DEG C, be put into 5g over dry cornstalk celluloses（Cellulose mass dryness fraction is
30%, therefore 5/30%=16.7g cornstalk celluloses are taken, wherein 11.7g is the weight of water）High degree of agitation 8min, makes cellulose
It is fully dissolved, dissolved cellulose solution centrifuges 30min under 15000rpm, collects supernatant, obtains cornstalk fibers
Plain lysate.
（4）The preparation of maize leaves active carbon nanoparticles
Maize leaves powder is carbonized 3.0h in 300 DEG C of Muffle furnaces, carbide be cooled to room temperature after using ball milling 72h,
Continuing the 12h that is carbonized in 300 DEG C of Muffle furnaces, carbonization material in drier is cooled to room temperature, is scattered in absolute ethyl alcohol again,
Magnetic agitation 72h, wherein quality of material are 1mg with absolute ethyl alcohol volume ratio:1mL；It is centrifuged under 15000rpm after the completion of immersion
35min collects supernatant, dry, obtains active carbon nanoparticles.
（5）The preparation of the full stalk regenerated cellulose of corn-active carbon nanoparticles blended gel film
Take step（4）In 1mg active carbon nanoparticles and 200mL steps（3）In cellulose dissolution liquid be uniformly mixed（The two
Than for 1mg:200mL）, a diameter of 20mm is poured into, depth is in the mold of 1mm, by the mold equipped with mixed liquor in 20% sulfuric acid bath
Middle submergence 180min, sample gradually form solidifying solid gel mould by viscous liquid, and film is removed from the molds, with deionized water into
Row washs repeatedly, is freeze-dried, and obtains the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of round corn.
（6）The character of the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of corn
Adsorption of metal ions assay method:It is a concentration of that the desiccant gel film of measure access 50mg is immersed in 1mL respectively
The Zn of 1mg/mL2+、Fe3+、Cd3+And Cu2+In standard solution, 72h is stood under 25 DEG C of water temperatures, after adsorption equilibrium, take out film, wipe
It wipes film surface layer liquid away, the content of beary metal adsorbed in film is detected using elemental analyser.
Blended gel film as obtained by above-mentioned reaction has higher metal adsorption capacity, to Zn2+、Fe3+、Cd3+And Cu2+
Adsorption capacity respectively reaches 480mg/g, 268mg/g, 289mg/g and 430mg/g.
Embodiment 4：It is specific to grasp based on the preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film
Make as follows：
（1）The melting process of maize straw
Stalk is by air-drying processing, wherein the water content for air-drying raw material is 20%, then air dry matter carries out leaf and stalk stripping
Processing, two parts raw material are crushed, are sieved with standard screen, take and sieve with 100 mesh sieve net respectively, but only the part of 200 mesh screens is two
Kind acceptable material.
（2）The extraction process of cellulose
Cellulose separation condition is:Potassium hydroxide dosage 35.0%, hydrogen peroxide use 25.0%, magnesium sulfate dosage
0.5%, anthraquinone dosage 0.20%, oxygen pressure 0.6MPa, material concentration for the treatment of 12.0%, reaction time 12.0h, treatment temperature
130℃。
The specific steps are:By the over dry cornstalk powder raw material of 10.0g（If it is 20.00% to air-dry raw material moisture, claim
12.5g is taken to air-dry material）With 17.5mL potassium hydroxide solutions（Concentration 200.0g/L), 25.0mL hydrogenperoxide steam generators（Concentration 100g/
L）, 1.0mL Adlerikas（Concentration 50g/L) and 0.020g anthraquinones mixing stir, add in total deionized water volume
For 27.3mL, mixed material is transferred to oxygen completely and takes off tank（Sealed pressure vessel tank）In, the oxygenation of 0.6MPa oxygen pressures amount
After 200s, sealing is put into rotatable heater, the primary delignification reaction 12.0h under the conditions of 120 DEG C；
Slurry after being disposed（That is gained cornstalk cellulose）It takes off and is transferred to completely in tank in 500 mesh slurry bag from oxygen,
Deionized water immersion, washing are carried out, until washings pH value is 7.0, it is pulp centrifuged after cleaning to slough excessive moisture, make cellulose
Mass dryness fraction is about 15.0% or so.
（3）Cornstalk cellulose course of dissolution
Cellulose dissolution condition is:Naoh concentration is 5.0% in lysate, urea concentration 20%, and lysate is first
It is cooled to -18 DEG C, the volume ratio of bone dry fiber quality amount and lysate is 1g:60mL.
Specifically dissolving step is:15.0g sodium hydroxides and 60g urea are weighed, with 271.7mL water mixed dissolutions, dissolving
After be put into refrigerating chamber lysate be cooled to -18 DEG C, be put into 5g over dry cornstalk celluloses（Cellulose mass dryness fraction is 15%,
Therefore 5/15%=33.3g cornstalk celluloses are taken, wherein 28.3g is the weight of water）High degree of agitation 20min carries out cellulose
Fully dissolving, dissolved cellulose solution centrifuge 20min under 12000rpm, collect supernatant, it is molten to obtain cornstalk cellulose
Solve liquid.
（4）The preparation of maize leaves active carbon nanoparticles
Maize leaves powder is carbonized 2.5h in 200 DEG C of Muffle furnaces, carbide be cooled to room temperature after using ball milling 50h,
Continuing the 10h that is carbonized in 200 DEG C of Muffle furnaces, carbonization material in drier is cooled to room temperature, is scattered in absolute ethyl alcohol again,
Magnetic agitation 48h, wherein quality of material are 5mg with absolute ethyl alcohol volume ratio:1mL；It is centrifuged under 10000rpm after the completion of immersion
20min collects supernatant, dry, obtains active carbon nanoparticles.
（5）The preparation of the full stalk regenerated cellulose of corn-active carbon nanoparticles blended gel film
Take step（4）In 1mg active carbon nanoparticles and 150mL steps（3）In cellulose dissolution liquid be uniformly mixed（The two
Than for 1mg:150mL）, a diameter of 15mm is poured into, depth is in the mold of 0.5mm, by the mold equipped with mixed liquor in 15% sulfuric acid
120min is submerged in bath, sample gradually forms solidifying solid gel mould by viscous liquid, and film is removed from the molds, and uses deionized water
It is washed, is freeze-dried repeatedly, obtain the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of round corn.
（6）The character of the full stalk regenerated cellulose blending active carbon nanoparticles gel mould of corn
Adsorption of metal ions assay method:It is a concentration of that the desiccant gel film of measure access 50mg is immersed in 1mL respectively
The Zn of 1mg/mL2+、Fe3+、Cd3+And Cu2+In standard solution, 72h is stood under 25 DEG C of water temperatures, after adsorption equilibrium, take out film, wipe
It wipes film surface layer liquid away, the content of beary metal adsorbed in film is detected using elemental analyser.
Blended gel film as obtained by above-mentioned reaction has higher metal adsorption capacity, to Zn2+、Fe3+、Cd3+And Cu2+
Adsorption capacity respectively reaches 480mg/g, 302mg/g, 291mg/g and 500mg/g.
Claims (3)
1. a kind of preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film, it is characterised in that by as follows
Step carries out：
1. the full stalk of corn carries out stalk after air-drying drying and leaf separation, shearing, grinding and stock of being sieved, stalk portion raw material use oxygen
Gas, hydrogen peroxide, potassium hydroxide and anthraquinone system handled, treated, and slurry with deionized water is impregnated, disperseed repeatedly
And washing, until it is neutral, after filtering out excessive moisture, cornstalk cellulose is made；
2. using sodium hydroxide or lithium hydroxide and urea or thiocarbamide, machine is carried out to cornstalk cellulose under cryogenic
The processing of tool stirring and dissolving, lysate are removed air and undissolved cellulose in liquid by centrifugation, obtain cellulose dissolution liquid；
3. the maize leaves heating carbonization after screening, the carbonization leaf after ball milling continue heating carbonization, ethyl alcohol impregnates dispersion, centrifugation
Supernatant is collected in separation, and after dry, active carbon nanoparticles are made；
4. active carbon nanoparticles are mixed with the cellulose dissolution liquid of step 2., pour into mold, and forming impregnated in sulfuric acid bath,
Gel mould is formed, film is washed repeatedly with deionized water, is freeze-dried, obtains the full stalk regenerated cellulose nano active of corn
Charcoal plural gel film.
2. the preparation method of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film according to claim 1,
It is characterized in that concrete operations are as follows：
1. the full stalk of corn after air-drying carries out leaf and stalk lift-off processing, and is sieved after crushing with 40~400 the polished standard screens, obtain
To powdered leaf and stalk two parts raw material；
2. cornstalk, potassium hydroxide, hydrogen peroxide and the anthraquinone after screening are sufficiently mixed after stirring evenly, it is transferred to oxygen completely
In de- tank, add in deionized water and adjust to 8.0~15.0% mass percent material concentration, it will in 0.1~0.8MPa oxygen pressure
After carrying out 60~300s of oxygenation under asking, sealing is put into rotatable heater and is reacted, and wherein potassium hydroxide dosage is over dry
The 20.0~50.0% of material quality, hydrogen peroxide use are the 10.0~35.0% of over dry material quality, and anthraquinone dosage is exhausted
The 0.05~0.5% of dry raw material quality, 5.0~15.0h of reaction time, 100~160 DEG C for the treatment of temperature；After being disposed, slurry
Tank taking-up is taken off from oxygen to be transferred to completely in 300~600 mesh slurry bag, is impregnated, washed with deionized water, until washings pH value
To 6.0~8.0, removing excessive moisture is centrifuged, cornstalk cellulose is made 10.0~30.0% in slurry mass dryness fraction；
3. first lithium hydroxide or sodium hydroxide and thiocarbamide or urea are dissolved in the water, make lithium hydroxide or hydrogen in aqueous solution
Sodium oxide molybdena mass percent concentration is 2.5~6.0%, and thiocarbamide or urea quality percent concentration are 8~25%, aqueous solution cooling
To after -20~-10 DEG C, add in cornstalk cellulose and 8~30min of high degree of agitation, wherein, cornstalk cellulose absolute dry mass with
The volume ratio of solution is 1g after cooling:10mL~1g:100mL, cellulose dissolution liquid centrifuges 10 under 7000~15000rpm~
30min, removes undissolved cellulose and bubble, and collection obtains cellulose dissolution liquid；
4. the maize leaves crushed heat 0.5~3.0h in 150~300 DEG C of Muffle furnaces, material utilizes ball milling after being cooled to room temperature
12~72h is ground, continues to heat 2~12h in 150~300 DEG C of Muffle furnaces, material is cooled to room temperature again in drier
Afterwards, it is scattered in absolute ethyl alcohol, 24~72h of magnetic agitation, wherein quality of material are 10mg with absolute ethyl alcohol volume ratio:1mL~
1mg:1mL；15~35min is centrifuged after the completion of immersion under 7000~15000rpm, collects supernatant, it is dry, obtain nanometer work
Property charcoal；
5. by active carbon nanoparticles and the cornstalk cellulose lysate of step 3. 1mg in proportion:10mL~1mg:200mL, mixing
Uniformly, mixed liquor is poured into mold, the mold equipped with mixed liquor submerges in the sulfuric acid bath of mass percent concentration 5~20%
Solidifying solid gel mould is removed from the molds, is washed repeatedly with deionized water by 10~180min, and freeze-drying obtains
The full stalk regenerated cellulose active carbon nanoparticles plural gel film of corn.
3. the preparation side of the full stalk regenerated cellulose of corn-active carbon nanoparticles plural gel film according to claim 1 or 2
Method, it is characterised in that：Magnesium sulfate is added in oxygen, hydrogen peroxide, potassium hydroxide and anthraquinone system, magnesium sulfate dosage is over dry
The 0.0~1.0% of material quality, and not equal to 0%.
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| CN106917309B (en) * | 2017-02-27 | 2018-03-06 | 昆明理工大学 | A kind of preparation method of corn stalk stalks of rice, wheat, etc. cellulose short-term training film |
| CN107128918A (en) * | 2017-05-26 | 2017-09-05 | 桂林电子科技大学 | A kind of preparation and its application of N doping porous active Carbon Materials |
| CN107261867B (en) * | 2017-08-10 | 2019-09-24 | 武汉纺织大学 | A kind of preparation method of super water-purifying filter film |
| CN107964118B (en) * | 2017-12-17 | 2019-05-21 | 王南南 | A kind of preparation method of epoxy resin composite conducting material special-purpose nanometer carbon fiber |
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